Pyridine → HCID 23339068、化合物

HRID 28134ノート

反応式

HRID 28134 の反応式
[CH3:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([CH3:8])[C:3]=1[NH:9][CH:10]1[CH2:15][CH2:14][N:13]([C:16]([O:18][CH2:19][CH3:20])=[O:17])[CH2:12][CH2:11]1.N1C=CC=CC=1.[C:27]1([CH2:33][C:34](Cl)=[O:35])[CH:32]=[CH:31][CH:30]=[CH:29][CH:28]=1>C1C=CC=CC=1>[CH3:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([CH3:8])[C:3]=1[N:9]([CH:10]1[CH2:15][CH2:14][N:13]([C:16]([O:18][CH2:19][CH3:20])=[O:17])[CH2:12][CH2:11]1)[C:34](=[O:35])[CH2:33][C:27]1[CH:32]=[CH:31][CH:30]=[CH:29][CH:28]=1

参加物

5

反応物 3

HCID 1049PyridineHCID 7679Phenylacetyl chlorideHCID 23338990HCID 23338990、化合物

生成物 1

HCID 23339068HCID 23339068、化合物

試薬・触媒・溶媒 1

HCID 241Benzene溶媒2 回

実験手順

To a stirred solution of 8 parts of ethyl 4-[(2,6-dimethylphenyl)amino]-1-piperidinecarboxylate in 4 parts of pyridine and 80 parts of benzene are added dropwise 7.7 parts of benzeneacetyl chloride in 40 parts of benzene. After the addition is complete, the whole is heated to reflux and stirred at reflux temperature for 3h.45. The reaction mixture is cooled and filtered. The benzene-phase is washed with water and then with sodium hydrogen carbonate solution and with water. After evaporation, an oily residue is obtained, which solidifies on triturating in 1,1'-oxybisethane, to yield 5 parts of ethyl 4-[N-(2,6-dimethylphenyl)-N-(phenylacetyl)amino]-1-piperidinecarboxylate; mp. 106° C.

後処理

  1. additionAfter the addition
  2. temperaturethe whole is heated
  3. temperatureto reflux
  4. temperatureat reflux temperature for 3h.45
  5. temperatureThe reaction mixture is cooled
  6. filtrationfiltered
  7. washThe benzene-phase is washed with water
  8. customAfter evaporation
  9. customan oily residue is obtained
  10. customon triturating in 1,1'-oxybisethane

出典と根拠

ORDレコード
ord-957f4cc3100f4fe3b632dfa5941fc43c
出典データセット
uspto-grants-1980_09
特許番号
US04225606

反応ノート

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